Process for dyeing or printing acetate silk



Patented Jan. 25,. 1927.;

UNITED, STATES osm srnnomn, PAUL max, m nunomr wnmnnmonn, or nnssau, enemy,

ASSIGNORS TO I. G. FARBENHWDUSTBE AKTIENGESELLSCHAIT, OF FBANKFOBT, I

GERMANY.

PROCESS FOR DY'EHI'G OB PRINTING ACETATE SILK.

80 Drawing. Application filed December 7, 1925, Serial No. 73,863Jand in Germany December 8, 1824 Acetate silk cannot be dyed at all or can added to the dye-bath or to the printing colbe dyed only in very limited degree with those'dyestufi's which are generally used for dyeing animal or vegetable fibres.

- Attempts have been made to' overcome the outstanding difiiculties by treating acetate silk superficially with an alkali or alkaline earth metal hydroxid so as to saponify its surface and thus give the latter an enhanced aflinity for dyestufis. The lustre of the fibre is, however, damaged by this process.

A process has been described in German specification No. 198,008 which consists in causing the acetyl cellulose or products made therefrom to absorb free amines and their derivatives or phenols and their derivatives from aqueous solutions. In so far as these compounds are not themselves dyestuffs, they may be converted on the fibre into dyestuffs in known manner. By this process there can be fixed on the acetate silk dyestuffs which dye cotton direct, or there may be produced on the fibre azo-dyestuifs or aniline black, and in the same manner other dyestufis, such as dihydroxyanthraquinones, can be brought on to the fibre, There are thus obtained indeed various tints but in most cases the lustre of the fibre is affected and the dyeings are notfast to rubbing. The process, moreover, offers no' guarantee for uniform dyeing throughout the fibre because the reactions which produce the dyeing occur mainl on the surface of the fibre. Since severa operations are necessary, the dyeing process becomes lengthy and costly.

By the present invention acetate silk can be dyed in various tints without afiecting the fibre, by treating it in presence of ammonia with an arylamine or a. derivative thereof under conditions such that coloured compounds are produced by an oxidation. Suitable for the process are not only bases such as 1:4-diaminobenzene. 4-amino-1-hydroxybenzene, but alsosuhstitution products,

such as dihydroxydiphenylamine, leuco-indophenols, the N-arylor N-alkyl-deriva'tives of 1:4diaminobenzene and 4-amino-1-hy-" droxybenzene. J Also nucleal substitution products ofthe, said compounds and others. Sucli bases may be used in intermixture with each other,- or withv hydroxy-aryl-com- Generally, the necessary oxidizing agent is our but in, some cases, as with the leucoindophenols, the compounds sufi'er auto-oxidation. As compared with the process of the aforesaid German specification, the process of the invention ofiers a considerable technical advance becauseit is simpler to carry through and produces full tints not obtainable .or only in part obtainable in other ways, and the dyeings are fast to rubbing. The acetate silk retains its lustre and its solubility in acetone.

The following examples illustrate the invention. V

Example 1..4: 4 dihydroxydiphenylamine is brought into solution with some Turkey red oil and addition of ammonia. The acetate silk is brought into the bath at about 40 C. and after half-an-hour is washed. There is obtained a brownish-red.

3:5"-dichloro-4-amino-4-hydroxydi henylamine dyes under like conditions b uish red. 4'-amino-4-hydroxydiphenylamine dyes strong clear violet.

p Ewample $3.4='-dimethylamino-4-hydroxydiphenylamiue is used as described in the preceding example. Thereby the acetate silk is dyed clear blue. By mixing this base with suitable compounds which yield yellow, there is obtained a green tint of great clearness.

Exam le 3.-10 kilos of acetate silk are introduce at ordinary temperature into a solution of- 500 grams of lz l-diaminobenzene in 250 litres of water, 5 litres of ammonia of 25 per cent strength and 20'litres of h drogen peroxide of 3 per cent strength; t e bath is heated gradually to 60 C; Washed and dried-artificial silk has a full brown colour which by after-treatment with a weak acetic acid solution of copper sulphate and alkali bichromate can be deepened. The dye-bath can be used again.

Example 4.10 kilos of acetate silk are -;tion of the dyein the silk is bronze to brown in colour. By a er-treatment with an acetic acid solution of copper sulphate and alkali bichromate there is obtained a deep violet brown.

-Ewample 5.10 kilos of acetate silk are dyed at a temperature gradually increasing to 50-60 C. in a liquor consisting of 300 grams of 2-para-hydroxyphenylaminonaphthalene, dissolved with aid of alkali in 250 litres of water, 3 kilos of ammonium chloride and 300 grams of potassium ferri-cyanide. The dyed silk is washed and dried. Salmon to reddish orange tints are produced.

Example 6'.-1O kilos of acetate silk are dyed at a temperature gradually rising to -50 C, in a liquor consisting of 300 grams of 4 4'-dihydroxydiphenylamine dissolved with aid of alkali in 250 litres of water, 3 kilos of ammonium chloride and 300 grams of potassium ferri-cyanide. The washed and dried silk is a full red.

Example 7.-10 kilos of acetate silk are dyed at a temperature gradually rising to 40 C. in a liquor consisting of 165 grams of 1:4-diaminobenzene, 180 grams of hydroxybenzene, 300 litres of water, 5-6 litres of ammonia of 25 per cent strength and 700 grams of potassium ferri-cyanide. The washed and dried silk is a deep luminous violet. Example 8.-10 kilos of acetate silk are dyed in a liquor consisting of 165 grams of 1:4-diaminobenzene, 360 grams of dimethylaminoben'zene, dissolved with acid of hydrochloric acid, 250 litres of water, 5-6 litres of ammonia of 25 per cent strength and 1 kilo of potassium ferri-cyanide. There is obtained a full violet dyeing.

Ewample .9.-10 kilos of acetate silk are treated at ordinary temperature in a liquor prepared from 300 litres of water, 360 grams of dimetnylaminobenzene dissolved in hydrochloric acid, 220 grams of t-amino-lhydroxybenzene hydrochloride, 5 litres of ammonia of 25 per cent strength and ,1 kilo of (potassium ferri-cyanide; The silk is dye a luminous pure blue.

Having thus fully described the nature of the said invention and the best means I know of carrying the same into practical effect,'I claim 1. A process of dyeing or printing acetate silkwhich process comprises treating the silk in presence of ammonia with an arylamine, which forms a coloured compound by oxidation in presence of ammonia.

2. A process for dyeing or printing acetate silk which process comprises treating the silk in presence of ammonia with a derivative of an arylamine, which forms a coloured compound by oxidation in presence of ammonia.

3. A process for dyeing or printing acetate silk, which process comprises treating the silk, in presence of ammonia and an oxidizing agent, with an arylamine which forms a coloured compound by oxidation in presence of ammonia.

4. A process for dyeing or printing acetate silk, which process comprises treating the silk, in presence of ammonia and an oxidiz ing agent, with a derii'ative of an arylamine, which forms a coloured compound by oxidation in presence of ammonia.

5. A process for dyeing or printing acetate silk, which process comprises treating the silk, in presence of ammonia and an hydroxy-aryl compound, with an arylaniine which forms a coloured compound by oxidation in presence of ammonia.

6. A process for dyeing or printing acetate silk, which process comprises treating the silk, in presence of ammonia and an hydroxy-aryl compound, with a deritative of an arylamine which forms a coloured compound by oxidation in presence of ammonia.

, 7. A process for dyeing or printing acetate silk, which process comprises treating the silk, in presence of ammonia, an oxidizing agent and an hydroxy-aryl compound, with an arylamine which forms a coloured compound by oxidation in presence of ammonia.

8. A process for dyeing or printing acetate silk, which process comprises treating the silk, in presence of ammonia, an oxidizing agent and an hydroxy-aryl compound, with a derivative of an arylamine which forms a coloured compound byoxidation in presence of ammonia.

In testimony whereof we afiix our-signatures.

OSKAR SPENGLER. a PAUL VIRCK. RUDOLF W'EIDENHAGEN. 

